Dissemination of gas CRM in China

Hai Wu
wuhai@nim.ac.cn

National Institute of Metrology (NIM), China

2016/7/27

14th workshop, APMP/TCQM GAWG

Mongolia, 26-28 July 2016
Outlines

• Administration of gas CRMs in China

• Inter-lab comparison on gas CRMs
• Gas CRM used for calibration of analyzers

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1- Administration of CRMs in China
◎ Traceability system of gas measurement

MRA

Developed by NIM KC, PR

National CRM

Calibration Procedures

Calibration/Measurement Results
By testing/calibration labs
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1- Administration of CRMs in China
◎ Administration of CRMs

4
1- Administration of CRMs in China
◎ Requirements for CRMs of Level 1 and 2
CRM Level 1 (GBW XXXX)
Producer Bodies qualified by AQSIQ.
Typically are metrological
research institutes, authority
labs or others
Characterization 1) By using absolute method of
technique highest accuracy;
2) Two methods of different
principles;
3) Multi-lab collaboration;
Stability Stable over ≥ 1 year;
Applications 1) Calibration of instrument;
2) Validation of method;
3) Validation of CRM Level 2;
4) Other applications
CRM Level 2(GBW(E) XXXX)
Bodies qualified by AQSIQ.
Typically are industries,
research institutes or others
1) Same techniques as used for
CRM Level 1;
2) Certification against CRM
Level 1;
Stable over several months;
1) Calibration of instrument;
2) Validation of method;
3) Routine measurement ;
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1- Introduction of CRMs in China
◎ Gas CRMs and producers CRM numbers: Level 1
-Level 1: ~150 NIM Other

-Level 2: ~1700
-RMP: ~150 8%

Gas CRMs of NIM

92%

24% Environment
Food
37%
Energy CRM numbers: Level 2
Safety NIM Other
3% Purity Gas
6% Medical
Forensic 6%
6% Others
6%
9%
9%

94%

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2- Inter-lab comparison on gas CRMs
• ILC is important for maintain the equivalence of gas CRMs
– RMP: 150
– CRM of level 2: 1700 kinds

• NIM’s role
– Coordinating ILC on gas
CRMs
– Link to CMC
– Sharing knowledge in order to
improve equivalence of national
CRMs

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2.1- ILC on CH4/air

– Methane alarmer subject to

compulsory verification CCQM-K82

– 0.5%mol/mol, 3%mol/mol
are the typical concentration
level at which verification
were conducted.

– En ratios of 95% of 30 CRMs within ±1

1.500 1.000

1.000

0.500

0.500
En值

En值
0.000 0.000
L0 4
L2 1
L1 0
L2 2
L0 2
L1 5
L1 2
L2 3
L2 0
L0 1
L1 6
L1 8
L2 8
L2 9
L2 7
L0 5
L2 6
L1 3
L3 0
L1 4
L0 3
L0 9
L0 7
L1 1
L0 8
L0 6
L1 9
L2 5

L15
L27
L16
L14
L22
L07
L01
L20
L24
L02
L13
L04
L19
L12
L28
L26
L18
L10
L17
L05
L09
L11
L21
L29
L30
L03
L25
L23
L06
L08
-0.500

-0.500

-1.000

-1.500 -1.000
实验室代码 实验室代码

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2.2- ILC on H2S CRMs
• H2S are typical sulfur-containing air pollutant in the air
• CRMs of (10~100)mol/mol are usually used to calibrate H2S detectors
• 12 RMP prepared CRM and sent to NIM for preparation comparison.
• En ratios of ~50% CRMs were not satisfied
– Most En ratio were below -1
– H2S adsorption effect onto cylinder surface may cause drop in concentration.

4
2
0
-2
En -4
-6 A B C D E F G H I J K
-8
-10
-12 系列1 系列2
-14
研制单位

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3- Gas CRMs establish traceability
• Mandatory verification based on Metrology Law
– Catalogue of working measurement instrument subject to compulsory
verification
• Include list of gas analyzers used in trade settlement, safety
protection, medical healthcare, and environmental monitoring
• Above analyzers be subject to periodical verification (compulsory
calibration, so called “verification”)
– MTCs (Measurement Technology Committee)
• Setting verification SOPs for each analyzer
– JJG 968 verification regulation of flue gas analyzer
stability, repeatability, indicate error(accuracy)…
• In which CRMs should be used

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3.1- CRMs establish traceability in IAQ measurement

IAQ standard Setting criteria for 13 air pollutants

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Traceability system of HCHO measurement
• HCHO standard generation system
– Basing on ISO 6145
– Dissemination range: 0-10ppm
– ACRM collaboration project:
trilateral comparison results proved
equivalence
– Used to calibrate HCHO analyzer

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Traceability system of O3 measurement

• Ozone measurement
– SRP41
• Established by NIST
• National primary standard
• Range: 0-1000ppb
• Participating in BIPM.QM-K1

– NIM O3 measurement standard

• Range 1：0-1000ppb
• Range 2：0-500ppm
(Sterilization device)
• JJG 1077-2012, verification
regulation for O3 analyzer

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3.2-Traceability system of exhaust gas measurement

• Vehicle emission measurement is mandatory

1999 GB I

2002
GB II

GB III
2005

2008 GB IV

2013
BEIJING V

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3.2-Traceability system of exhaust gas measurement

• JJG 688-2007
Calibrated parameters:
Propane, carbon monoxide, carbon dioxide
Nitrogen monoxide, oxygen

CCQM-K3
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3.3-Traceability system of flue gas measurement

• CRMs for flue gas measurement

– NO: 10-100 µmol/mol
– SO2: 20-200 µmol/mol
– CO: 10-100 µmol/mol
– CO2: 100-160 mmol/mol
– C3H8: 1-10 µmol/mol
– balance：N2

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3.4-Traceability system of exhaust gas measurement
CCQM-K23b -- i-Butane

5.0%
4.0%
3.0%

Relative deviation (%)

2.0%
1.0%
0.0%
-1.0%
-2.0%
-3.0%
-4.0%
-5.0%

BAM

GUM

KRISS
OMH
SMU

NRCCRM
NPL

NMi VSL
CMI

CENAM

CEM

NMIA

IPQ

INMETRO

NMIJ
VNIIM
Laboratory

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3.5- Gas CRM addresses industry need

 Address need from State GRID Corporation

 Setting up criteria of diagnosis for GIS based on
the measurement results.

 CRM for measuring decomposition products of GIS

SF6
 SO2
 SO2F2
 SOF4
 HF
 C3H8
 CO
 …

 CRM needed when evaluating the performance of

SF6 analyzers
summary
• Gas CRM plays important role in establishing the traceability
of calibration/measurement results
• Around 150 RMPs serve over 1800 kind of gas CRMs in
China. NIM as the NMI take the responsibility of establishing
international equivalence of gas CRMs.
• ILC is an important manner to provide external QA to the.
RMP
• Some gas analyzers of special applications are subject to
mandatory verification in China, in order to ensure the
traceability of measurement results.

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Thanks for your attention.

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